CN1433567A - Post chemical-mechanical planarization (CMP) cleaning composition - Google Patents
Post chemical-mechanical planarization (CMP) cleaning composition Download PDFInfo
- Publication number
- CN1433567A CN1433567A CN01810723A CN01810723A CN1433567A CN 1433567 A CN1433567 A CN 1433567A CN 01810723 A CN01810723 A CN 01810723A CN 01810723 A CN01810723 A CN 01810723A CN 1433567 A CN1433567 A CN 1433567A
- Authority
- CN
- China
- Prior art keywords
- solution
- ascorbic acid
- cleaning
- cleaning solution
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000004140 cleaning Methods 0.000 title claims abstract description 115
- 239000000203 mixture Substances 0.000 title claims description 43
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 94
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims abstract description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 39
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 38
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 38
- 239000000758 substrate Substances 0.000 claims abstract description 34
- 238000005260 corrosion Methods 0.000 claims abstract description 33
- 230000007797 corrosion Effects 0.000 claims abstract description 33
- 238000004377 microelectronic Methods 0.000 claims abstract description 20
- 239000003112 inhibitor Substances 0.000 claims abstract description 16
- 150000001412 amines Chemical class 0.000 claims abstract description 12
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 11
- 125000001453 quaternary ammonium group Chemical group 0.000 claims abstract description 10
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 38
- 239000012141 concentrate Substances 0.000 claims description 30
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 239000003513 alkali Substances 0.000 claims description 13
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 10
- 229960001484 edetic acid Drugs 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- CIWBSHSKHKDKBQ-DUZGATOHSA-N D-isoascorbic acid Chemical compound OC[C@@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-DUZGATOHSA-N 0.000 claims description 7
- 239000002211 L-ascorbic acid Substances 0.000 claims description 7
- 235000000069 L-ascorbic acid Nutrition 0.000 claims description 7
- 235000010352 sodium erythorbate Nutrition 0.000 claims description 7
- 150000005622 tetraalkylammonium hydroxides Chemical group 0.000 claims description 7
- JPIGSMKDJQPHJC-UHFFFAOYSA-N 1-(2-aminoethoxy)ethanol Chemical compound CC(O)OCCN JPIGSMKDJQPHJC-UHFFFAOYSA-N 0.000 claims description 6
- CIWBSHSKHKDKBQ-SZSCBOSDSA-N 2-[(1s)-1,2-dihydroxyethyl]-3,4-dihydroxy-2h-furan-5-one Chemical compound OC[C@H](O)C1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-SZSCBOSDSA-N 0.000 claims description 6
- OPKOKAMJFNKNAS-UHFFFAOYSA-N N-methylethanolamine Chemical compound CNCCO OPKOKAMJFNKNAS-UHFFFAOYSA-N 0.000 claims description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- LHIJANUOQQMGNT-UHFFFAOYSA-N aminoethylethanolamine Chemical compound NCCNCCO LHIJANUOQQMGNT-UHFFFAOYSA-N 0.000 claims description 6
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 6
- 229940043237 diethanolamine Drugs 0.000 claims description 6
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 4
- 229930003268 Vitamin C Natural products 0.000 claims description 4
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 4
- 235000019154 vitamin C Nutrition 0.000 claims description 4
- 239000011718 vitamin C Substances 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- -1 monoethylanolamine Chemical compound 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 122
- 239000010949 copper Substances 0.000 description 50
- 229910052802 copper Inorganic materials 0.000 description 40
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 39
- 235000012431 wafers Nutrition 0.000 description 29
- 238000000089 atomic force micrograph Methods 0.000 description 25
- 238000000034 method Methods 0.000 description 20
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 18
- 238000004070 electrodeposition Methods 0.000 description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 13
- 229910052751 metal Inorganic materials 0.000 description 11
- 239000002184 metal Substances 0.000 description 11
- 238000002474 experimental method Methods 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 10
- 239000004065 semiconductor Substances 0.000 description 10
- 235000004515 gallic acid Nutrition 0.000 description 9
- 229940074391 gallic acid Drugs 0.000 description 9
- 230000008569 process Effects 0.000 description 8
- 239000002002 slurry Substances 0.000 description 8
- 239000012535 impurity Substances 0.000 description 7
- 238000005498 polishing Methods 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 6
- 230000003321 amplification Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 238000003199 nucleic acid amplification method Methods 0.000 description 6
- 238000007598 dipping method Methods 0.000 description 5
- 239000008187 granular material Substances 0.000 description 5
- 239000000523 sample Substances 0.000 description 5
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 229920002120 photoresistant polymer Polymers 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Substances C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229960004643 cupric oxide Drugs 0.000 description 3
- 239000003989 dielectric material Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000002738 chelating agent Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000011440 grout Substances 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 150000002484 inorganic compounds Chemical class 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- SIQZJFKTROUNPI-UHFFFAOYSA-N 1-(hydroxymethyl)-5,5-dimethylhydantoin Chemical compound CC1(C)N(CO)C(=O)NC1=O SIQZJFKTROUNPI-UHFFFAOYSA-N 0.000 description 1
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000005269 aluminizing Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- LIWAQLJGPBVORC-UHFFFAOYSA-N ethylmethylamine Chemical compound CCNC LIWAQLJGPBVORC-UHFFFAOYSA-N 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- DZKDPOPGYFUOGI-UHFFFAOYSA-N tungsten dioxide Inorganic materials O=[W]=O DZKDPOPGYFUOGI-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
- H01L21/0206—Cleaning during device manufacture during, before or after processing of insulating layers
- H01L21/02063—Cleaning during device manufacture during, before or after processing of insulating layers the processing being the formation of vias or contact holes
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/38—Cationic compounds
- C11D1/62—Quaternary ammonium compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0073—Anticorrosion compositions
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/28—Heterocyclic compounds containing nitrogen in the ring
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/30—Amines; Substituted amines ; Quaternized amines
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/265—Carboxylic acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3209—Amines or imines with one to four nitrogen atoms; Quaternized amines
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3218—Alkanolamines or alkanolimines
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3245—Aminoacids
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3254—Esters or carbonates thereof
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/42—Stripping or agents therefor
- G03F7/422—Stripping or agents therefor using liquids only
- G03F7/425—Stripping or agents therefor using liquids only containing mineral alkaline compounds; containing organic basic compounds, e.g. quaternary ammonium compounds; containing heterocyclic basic compounds containing nitrogen
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
- H01L21/02068—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers
- H01L21/02074—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers the processing being a planarization of conductive layers
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/22—Electronic devices, e.g. PCBs or semiconductors
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Cleaning Or Drying Semiconductors (AREA)
- Detergent Compositions (AREA)
Abstract
The present invention discloses a cleaning solution for cleaning microelectronic substrates, particularly for post-CMP or via formation cleaning. The cleaning solution comprises a quaternary ammonium hydroxide, an organic amine, a corrosion inhibitor, and water. A preferred cleaning solution comprises tetramethylammonium hydroxide, monoethylanolamine, ascorbic acid, and water with the alkalinity of the cleaning solution greater than 0.073 milliequivalents base per gram of solution.
Description
Invention field
Generally speaking, the present invention relates to post-chemical mechanical polishing (post chemical-mechanicalpolishing, back CMP) washing and cleaning operation field, more particularly, the present invention relates to the back CMP cleaning solution of microelectronic substrate.
Background of invention
The method of making semiconductor device at present is the rapid process of multistep of a complexity.Chemical mechanical planarization (CMP) method is the known technology in most of advanced persons' the semiconductor operation now, is used for being used for various base planization during less than 0.35 micron device in the production physical dimension.
The CMP method is included in the Boping substrate that faces toward wetting polished surface clamping and rotation semi-conducting material under controlled chemistry, the pressure and temperature condition.With the chemical grout that contains polishing agent such as aluminium oxide (alumina) or silicon dioxide (silica) as abrasive material.Also contain in the chemical grout and select to be used in each surperficial chemical substance of course of processing etching substrates.The method of machinery and chemistry being removed material in polishing process combines and can reach effect with the super complanation in surface.
But the CMP method has stayed impurity (contamination) on semiconductor substrate surface.This impurity is by may be by constituting from the abrasive grain of polishing slurries and the reactive chemical that adds polishing slurries that aluminium oxide or silicon dioxide are formed.Impurity layer may also comprise the product of polishing slurries and polished surface.Reduce for fear of device reliability, and, must before semiconductor substrate is carried out following process, remove these impurity for fear of introducing the defective that productive rate is reduced.Therefore people have developed the back CMP cleaning solution of the substrate surface that is used to clean the residual layer of CMP.
Use alkaline solution to carry out back CMP cleaning traditionally based on ammonium hydroxide.Present most of CMP is used on the surface that contains aluminium, tungsten, tantalum and oxide.
But when making semiconductor, copper becomes day by day produces interconnected material.Copper is replacing aluminium as the metal of making these devices.Traditional back CMP method is not enough to clean copper containing surfaces.Copper, cupric oxide and serous granule are to carry out being present in the lip-deep impurity of copper after the CMP technology.The copper surface can be dispersed in silicon and the silicon dioxide fast.Therefore must remove the lip-deep copper of all wafers to prevent component failure.
Invalid to aluminium oxide and the effective back of silicon-dioxide-substrate CMP technology CMP cleaning solution traditionally to copper containing surfaces.Copper is easy to be subjected to the destruction of these cleaning solutions.In addition, the cleaning efficiency of present back CMP cleaning solution can not be accepted.
Disclose a kind of cleaning solution that is used for semiconductor device in the United States Patent (USP) 5863344 of Nam, this solution contains tetramethylammonium hydroxide, acetate and water.The acetate that preferably contains in this solution and the volume ratio of tetramethylammonium hydroxide are about 1 to about 50.
Disclose a kind of moisture stripping composition that is used for the organic and inorganic compound of cleaning base plate in the United States Patent (USP) 5597420 of Ward, these organic and inorganic compounds can not corrode or dissolve the metallic circuit in the substrate.Disclosed Aquo-composition preferably contains the monoethanolamine of 70-95wt% and corrosion inhibitor such as catechol, 1,2,3,-thrihydroxy-benzene or the gallic acid of about 5wt%.
Disclose a kind of cleaning combination in the United States Patent (USP) 5709756 of Ward, said composition contains the azanol of the 25-48wt% that has an appointment, ammonium fluoride and the water of 1-20wt%.The pH of this solution is greater than 8.This solution also can contain corrosion inhibitor such as gallic acid, catechol or 1,2,3,-thrihydroxy-benzene.
A kind of aqueous alkaline cleaning solution that is used for the cleaning microelectronic substrate is disclosed in people's such as Hardi the United States Patent (USP) 5466389.This cleaning solution contains the basic component of non-metallic ion such as quaternary ammonium hydroxide (high-load be 25wt%), non-ionic surface active agent (high-load be 5wt%) and pH regulates component such as acetate, and pH regulates component and is used for pH is controlled in the 8-10 scope.
Disclose among people's such as Schwartzkopf the European patent 0647884A1 and contained the photoresist release agent that is useful on the reducing agent that reduces corrosion of metals.At the alkaline constituents that contains that is used for controlling corrosion of metals, this patent has been used ascorbic acid, gallic acid, 1,2,3,-thrihydroxy-benzene.
Be issued to the novel ascorbic acid derivates that discloses in people's such as Satoh the United States Patent (USP) 5143648 as antioxidant, introduce this patent herein as a reference.
Disclose a kind of moisture stripping composition in the United States Patent (USP) 5563119 of Ward, said composition is made up of alkanolamine, tetraalkylammonium hydroxide and corrosion inhibitor, and said composition is used for cleaning the organic remains of inorganic substrate of aluminizing.
Need a kind of back CMP cleaning combination that is used for copper containing surfaces now.Back CMP cleaning combination like this need basically can be effectively with particle removals all in fact in the target surface and can prevent to containing the corrosion of copper base.Back CMP cleaning combination so also needs to avoid the destruction to the process equipment that uses in the CMP technology of back.Back CMP cleaning combination so also should be economical, can be in very wide temperature range effective operation.Back CMP cleaning combination so also should be applicable to the washing and cleaning operation after the CMP technology of utilizing aluminium oxide or silicon dioxide based slurries.
Summary of the invention
The present invention is a kind of moisture cleaning solution that is used for the cleaning microelectronic substrate, and this solution comprises the quaternary ammonium hydroxide that is selected from tetraalkylammonium hydroxide, and alkyl wherein contains C
1-C
10A kind of or C in the atom
1-C
10Combination in the atom; Be selected from monoethanolamine, amino ethyl ethanolamine, N-methylaminoethanol, amino ethoxy ethanol, diethanol amine, triethanolamine, C
2-C
5The organic amine of alkanolamine and composition thereof; Be selected from the corrosion inhibitor of ascorbic acid, L (+)-ascorbic acid, arabo-ascorbic acid, ascorbic acid derivates, citric acid, ethylenediamine tetra-acetic acid (EDTA), BTA and composition thereof.The basicity of this solution is greater than 0.073 milliequivalent alkali/gram solution.
Therefore, one aspect of the present invention is a kind of cleaning solution that is used for the cleaning microelectronic substrate, and this cleaning solution comprises: the quaternary ammonium hydroxide that is selected from tetraalkylammonium hydroxide of 0.05-12.4wt%, alkyl wherein contains C
1-C
10A kind of or C in the atom
1-C
10Combination in the atom; 0.2-27.8wt% is selected from monoethanolamine, amino ethyl ethanolamine, N-methylaminoethanol, amino ethoxy ethanol, diethanol amine, triethanolamine, C
2-C
5The polarity organic amine of alkanolamine and composition thereof; The corrosion inhibitor that is selected from ascorbic acid (vitamin C), L (+)-ascorbic acid, arabo-ascorbic acid, ascorbic acid derivates, BTA, citric acid, ethylenediamine tetra-acetic acid (EDTA) and composition thereof of effective dose; Water with surplus.The basicity of this solution is greater than 0.073 milliequivalent alkali/gram solution.
One aspect of the present invention is a kind of cleaning solution that is used for the cleaning microelectronic substrate, and this solution comprises: a) tetramethylammonium hydroxide, b) monoethanolamine, c) ascorbic acid and deionized water.The basicity of this solution is greater than 0.073 milliequivalent alkali/gram solution.Preferably, the amount of tetramethylammonium hydroxide is extremely about 1.25wt% of about 0.15wt% in the cleaning solution, and the amount of monoethanolamine is extremely about 2.25wt% of about 0.2wt% in the cleaning solution, and the amount of ascorbic acid is that about 0.10wt% is to about 0.9wt% in the cleaning solution.
Another aspect of the present invention is a kind of cleaning solution that is used for the cleaning microelectronic substrate, this cleaning solution is made up of the concentrate of 1.5-12.5wt% and the deionized water of 87.5-98.5wt% basically, this concentrate is made up of following substances: the quaternary ammonium hydroxide that is selected from tetraalkylammonium hydroxide of 3.0-12.4wt%, alkyl wherein contains C
1-C
10A kind of or C in the atom
1-C
10Combination in the atom; 5.0-27.8wt% is selected from monoethanolamine, amino ethyl ethanolamine, N-methylaminoethanol, amino ethoxy ethanol, diethanol amine, triethanolamine, C
2-C
5The polarity organic amine of alkanolamine and composition thereof; Corrosion inhibitor that is selected from ascorbic acid (vitamin C), L (+)-ascorbic acid, arabo-ascorbic acid, ascorbic acid derivates, BTA, citric acid, ethylenediamine tetra-acetic acid (EDTA) and composition thereof and the surplus of 2.0-10.9wt% are water.The basicity of this solution is greater than 0.073 milliequivalent alkali/gram solution.
Another aspect of the present invention is that a kind of preparation is used for the concentrate composition that the cleaning solution of cleaning microelectronic substrate is used.This concentrate composition comprises the tetramethylammonium hydroxide of about 3.0wt% to about 12.4wt%, and about 5wt% is to the monoethanolamine of about 27.8wt%, and about 2.0wt% is to ascorbic acid and the balance of deionized water of about 10.4wt%.The preparation method of cleaning solution will extremely mix with deionized water near the concentrate of 100wt% at least about 1.5wt%.Also can no longer directly use this concentrate with the water mixing.
The accompanying drawing summary
Fig. 1 is that the sweep limits of its amplification is 10 μ m * 10 μ m at the atomic force micrograph (AFM) on the electrochemically depositing copper surface of substrate top polishing.
Fig. 2 is the atomic force micrograph (AFM) with the wafer shown in Figure 1 of solution-treated of the present invention, and the sweep limits of its amplification is 10 μ m * 10 μ m.
Fig. 3 is that the sweep limits of its amplification is 10 μ m * 10 μ m with the atomic force micrograph (AFM) of the copper sample shown in Figure 1 of another kind of composition cleaning of the present invention.
Fig. 4 is that the sweep limits of its amplification is 10 μ m * 10 μ m with the atomic force micrograph (AFM) of the copper sample shown in Figure 1 of different components processing of the present invention.
Fig. 5 is that the sweep limits of its amplification is 10 μ m * 10 μ m with the atomic force micrograph (AFM) of the through hole before the compositions-treated of the present invention.
Fig. 6 is the atomic force micrograph (AFM) with the through hole shown in Figure 5 after the compositions-treated of the present invention, and the sweep limits of its amplification is 10 μ m * 10 μ m.
Fig. 7 is the datagram of expression with granule number on the wafer before and after the composition cleaning of the present invention.
Fig. 8 is the scintigram with granule number on the wafer before and after the solution cleaning of the present invention.
Detailed Description Of The Invention
The invention provides a kind of cleaning solution that carries out the cupric microelectronic substrate after the CMP technique for cleaning. Generally the cleaning that contains copper base after the CMP technique is called " rear CMP copper cleans (post CMP copper clean) ". " cupric microelectronic substrate " should be interpreted as the substrate surface for the production of microelectronic component, integrated circuit or computer chip in this article, wherein substrate contains the cupric component. The cupric component can comprise such as the metal interconnection that mainly is copper or copper alloy (metallic interconnect). Should be understood that the microelectronic component surface can also be made of such as TiN, Ta, TiW and silica as the copper diffusion barrier layer metal semi-conducting material. The cupric microelectronic substrate generally contains the copper of the 1-100% that has an appointment, and is interconnected comprising copper.
In the process of making microelectronic substrate such as semiconductor wafer, cleaning solution of the present invention can be used for any washing and cleaning operation. It should be noted that most that such cleaning suitable application area comprises rear through hole shaping (post-Via formation) and rear CMP technique. Many steps that need complanation are arranged when making traditional semiconductor chip, then remove the residual materials that planarization technology produces.
Cleaning solution of the present invention comprises the water of quaternary ammonium hydroxide, organic amine, corrosion inhibitor and surplus. Quaternary ammonium hydroxide is selected from tetraalkylammonium hydroxide (TMAH), and alkyl wherein contains C1-C
10A kind of or C in the atom1-C
10Combination in the atom. The amount of quaternary ammonium hydroxide in cleaning solution is that about 0.05wt% is to about 12.4wt%.
The polarity organic amine is selected from monoethanolamine (MEA), amino ethyl ethanolamine, N-methylaminoethanol, amino ethoxy ethanol, diethanol amine, triethanolamine, C2-C
5Alkanolamine and composition thereof. The amount of polarity organic amine in cleaning solution is that about 0.2wt% is to about 27.8wt%.
Corrosion inhibitor is selected from ascorbic acid, L (+)-ascorbic acid, arabo-ascorbic acid, ascorbic acid derivates, citric acid, BTA and composition thereof. The amount of corrosion inhibitor in cleaning solution is that about 0.2wt% is to about 10.9wt%. The effective cleaning surface can be removed from the surface cupric oxide and other impurity when wishing to reach best etching extent. Therefore, in order to reach optimal cleaning effect, this technique usually makes wafer surface produce a small amount of copper loss and loses, but can keep the electrical property of wafer.
The basicity of cleaning solution of the present invention is greater than 0.073 milliequivalent alkali/gram solution.A kind of concentrate composition that provides in one embodiment of the invention can dilute the back as cleaning solution.The advantage of concentrate composition of the present invention or " concentrate " is to allow user such as CMP process engineer that concentrate is diluted to desirable strength and basicity.The concentrate of product has the longer pot-life, is easier to transportation and storage.
Ascorbic acid and derivative thereof are widely used as antioxidant in food and medicine.People find that also they are suitable corrosion inhibitors for the metal or metal alloy that is present in moisture or the solvent environment.Ascorbic acid of the present invention and other component are easy to be purchased.
An important feature of cleaning solution of the present invention is to have a small amount of nonaqueous component (not being the component of water) in the solution.This has very big economic interests, because can prepare effective cleaning solution more economically, this point is very important, because the consumption of back CMP cleaning solution is very big.
Concentrate of the present invention preferably includes the TMAH of about 3.0-12.4wt%, and about 5.0wt% is to the MEA of about 27.8wt%, and about 2.0wt% is to the ascorbic acid of about 10.4wt% and the water of surplus (preferred deionized water).
In addition, concentrate of the present invention also can contain the chelating agent that further prevents the unwanted metal impurities of deposition on wafer surface.In said preparation, also can introduce the known metal chelating agent that is used for Zn, Cu, Ni, Fe etc.Everybody knows that also the metal protection ability of corrosion inhibitor is relevant with the complex compound formation performance that organic complex forms agent in many cases.
Be used for back CMP after concentrate of the present invention preferably dilutes and clean, method is to add deionized water, is about 1.5wt% about 12.5wt% extremely of the cleaning solution of preparation up to concentrate.Cleaning solution of the present invention can be from ambient temperature cleaning microelectronic substrate to about 70 ℃ temperature.Generally everybody can both understand cleaning performance and raises with temperature and improve.
As mentioned above, the basicity of cleaning solution of the present invention is greater than 0.073 milliequivalent alkali/gram solution.The basicity of cleaning solution of the present invention is remained greater than about 0.091 milliequivalent alkali/gram solution.
Cleaning solution of the present invention has reached generally accepted industrial cleaning performance standard in the back CMP application.The general industrial washing standard be for the 200mm wafer on the substrate wafer granularity greater than 0.2 micron granule number less than 20, and the border of 5mm is got rid of.
Cleaning solution of the present invention does not need surfactant when preparation, but does not get rid of the application of surfactant in specific field.
When using cleaning solution of the present invention, can use many traditional cleaning means, these cleaning means comprise Verteq single-chip megasonic Goldfinger, the wet in batches bench system of the DDS of OnTrak system (two-sided scrubber), the spraying rinsing of SEZ single-chip and Megasonic.
Cleaning solution of the present invention can successfully be applied on the surface of cupric, tungsten and/or silicon dioxide.
As mentioned above, a kind of application process of cleaning solution of the present invention is that through hole cleans.Through hole is the hole that is etched in the microelectronic substrate, and these holes are the passages that connect metal level.Produce through hole with the gas phase etchant etching substrate surface.Substrate generally is dielectric material such as fluorinated silica glass (FSG).After finishing, etch process must remove the residue that remains on substrate surface and the through-hole wall.Residue is commonly referred to " lateral wall polymer ", is on the vertical wall of through hole because people also find these residues.Etch residue also can be positioned at via bottoms, metal top.Cleaning solution of the present invention can not react with the dielectric material that exposes and can the dielectric material that expose do not exerted an influence yet.
The following examples only are for illustration the present invention, rather than limit the present invention.
Experimentize to estimate the relative cleaning performance of the different back CMP cleaning solutions of forming.The method for preparing cleaning solution is with a kind of the mixing in deionized water, TMAH, ascorbic acid and the three kinds of amines (MEA, azanol or N-monoethanolamine).The composition of the cleaning solution of preparation is shown in table 1.In order to reach the purpose of contrast, prepare two kinds of cleaning solutions in addition: solution 10 is NH that 1.7wt% is arranged in deionized water
4OH, solution 11 are NH of 1: 2: 10
4OH: H
2O
2: H
2O.
Carry out " dipping experiment " with the micro-slide of prewashed Fisher 12-550-10.In following step, all dipping processs all carried out for 5 seconds, and all handled with plastic clamp.Specimen slides at first is immersed in the CMP oxide slurries (Ultraplane P-1500), be immersed in then in the 250ml deionized water, be immersed in then in the W-CMP slurries (1: 1 dilution of Ultraplane-MC W CMP alkali and deionized water), then each slide glass is immersed in the 250ml deionized water, is immersed in the cleaning solution then.Then each slide glass is immersed in the 100ml deionized water, is immersed in then in another deionization water-bath that separates.Slide glass is hung, under environmental condition, dry.After the experiment, all deionization water-baths all will be replaced as new each time.
With residual CMP slurries is foundation, and from visually estimating dry slide glass, evaluation criterion is the turbidity on the observed slide glass.These dry slide glasses are compared, carry out classification from best (1) to the poorest (11) then.
The results are shown in table 1.
| The experiment of Table I contrast dipping | |||||||
| Amine | ??TMAH ??(wt％) | Amine (wt%) | Ascorbic acid (wt%) | Gallic acid (wt%) | Titration alkalinity milliequivalent/gram solution | Classification relatively | |
| ??1 | ??MEA | ????0.5 | ???0.9 | ?????0.2 | ????- | ?????0.191 | ????1 |
| ??2 | ??MEA | ????0.5 | ???0.9 | ?????0.35 | ????- | ?????0.182 | ????2 |
| ??3 | ??MEA | ????0.5 | ???0.9 | ??????- | ???0.35 | ?????0.182 | ????3 |
| ??4 | ??NMEA | ????0.5 | ???0.9 | ?????- | ???0.35 | ?????0.154 | ????4 |
| ??5 | ??MEA | ????0.5 | ???0.9 | ?????- | ???0.1 | ?????0.196 | ????5 |
| ??6 | ??HA | ????0.66 | ???0.3 | ?????- | ??0.233 | ?????0.235 | ????6 |
| ??7 | ??HA | ????0.66 | ???0.6 | ?????- | ??0.233 | ?????0.284 | ????7 |
| ??8 | ??HA | ????0.33 | ???0.3 | ?????- | ??0.467 | ?????0.122 | ????8 |
| ??9 | ??HA | ????0.33 | ???0.6 | ?????- | ??0.467 | ?????0.171 | ????9 |
| ??10 | ???- | ????- | ????- | ????- | ?????0.485 | ????10 | |
| ??11 | ???- | ????- | ????- | ????- | ?????NA | ????11 | |
These results show: the preferred embodiments of the invention performance best (that is solution 1 and 2).All solution of the present invention all cleaning solution performance (solution 10 and 11) than prior art are good.
Estimate the corrosive nature of cleaning solution (A-G) to copper.Solution A is made up of (L)-ascorbic acid and the balance of deionized water of TMAH, the 0.35wt% of MEA, the 0.5wt% of 0.9wt%.Solution B is made up of (L)-ascorbic acid and the balance of deionized water of TMAH, the 0.18wt% of MEA, the 0.5wt% of 0.9wt%.Solution C is made up of the MEA of 0.9wt% and the water of surplus.Solution D is made up of the gallic acid of TMAH, the 0.35wt% of MEA, the 0.5wt% of 0.9wt% and the water of surplus.Solution E is made up of the gallic acid of TMAH, the 0.18wt% of MEA, the 0.5wt% of 0.9wt%, the BTA of 0.18wt% and the water of surplus.Solution F is a buffered HF solution.Solution G is the NH of 1.7wt%
4The OH aqueous solution.Obtain the copper sheet of even length and width from electrochemical deposition (ECD) the copper wafer (partially polished) of full wafer, under environmental condition, copper sheet placed the sample cleaning solution 2 minutes that 200ml stirs then.Then the copper wafer is taken out from cleaning solution, use rinsed with deionized water, use nitrogen drying then.The change color of range estimation copper wafer and the gloss that loses.The two all is the proof that copper is corroded.Copper wafer to these processing carries out the micro-test of atomic force (AFM), tests its surface corrosion situation.
Corrosion results is shown in Table II.
| Table II corrosion experiment data | |||
| Composition | Substrate | Experimental technique | The result |
| Cu (ECD), partially polished | ???AFM | Pitting (pitting) slightly after the RMS=0.8 polishing | |
| Solution A | Cu (ECD), partially polished | ???AFM | The pitting of RMS=1.0 minimum, minimum Cu corrosion |
| Solution B | Cu (ECD), partially polished | ???AFM | The pitting of RMS=1.1 minimum, minimum Cu corrosion |
| Solution C | Cu (ECD), partially polished | ???AFM | RMS=3.4 is pitting slightly, moderate Cu corrosion |
| Solution D | Cu (ECD), partially polished | ???AFM | RMS=3.5 is pitting slightly, moderate Cu corrosion |
| Solution E | Cu (ECD), partially polished | ???AFM | The RMS=NA surface is by the BTA modification |
| Solution F | Cu (ECD), partially polished | ???AFM | The pitting of RMS=1.3 minimum, slight Cu corrosion |
| Solution G | Cu (ECD), partially polished | ???AFM | RMS=3.8 is pitting slightly, moderate Cu corrosion |
*The r.m.s. roughness that RMS=AFM measures.
Data in the Table II show: the copper corrosion barrier propterty of the preferred embodiments of the invention (solution A) is very good.The different concentration differences that are corrosion inhibitor of solution A and B.Other all solution are compared with this preferred embodiment can both cause a large amount of copper surface corrosions.Solution G has just removed lip-deep copper oxide, and therefore slight roughening takes place.
Fig. 1-4 illustrates embodiment and the RMS coarseness data with AFM scanning, wherein, Fig. 1 is untreated electrochemical deposition (ECD) copper wafer, Fig. 2 is the same ECD copper wafer that is immersed in the solution A, Fig. 3 is the ECD copper wafer that is immersed in the solution B, and Fig. 4 is the ECD copper wafer that is immersed in by in the gallic acid of TMAH, the 0.18wt% of MEA, the 0.5wt% of 0.9wt% and the solution that excess water is formed.
Prepare a series of cleaning solutions, estimate the relation of TMAH, MEA and ascorbic acid in the moisture cleaning solution.With the various combined preparation cleaning solutions of TMAH, MEA, ascorbic acid and deionized water, making TMAH concentration is 0.0wt%-0.5wt%; The concentration of MEA is 0wt%-0.9wt%; The concentration of ascorbic acid is 0wt%-0.35wt%; The surplus of solution is a deionized water.The experimental solutions of preparation is shown in Table III.Also the cleaning solution that will prepare according to the experimental procedure evaluation of embodiment 2 is to the copper corrosion performance of copper sheet.
The results are shown in Table III.
| Table III | |||||||
| Composition | ?????A | ????B | ????C | ????D | ????E | ????F | ????G |
| TMAH(wt％) | ????0.5 | ????X | ????X | ????0.5 | ????0.5 | ????X | ????0.5 |
| MEA(wt％) | ????0 | ????0.9 | ????X | ????0.9 | ????X | ????0.9 | ????0.9 |
| Ascorbic acid (wt%) | ????X | ????X | ???0.35 | ????X | ???0.35 | ???0.35 | ???0.35 |
| Water (wt%) | ???99.50 | ??99.10 | ???99.65 | ??98.60 | ??99.15 | ??98.75 | ??98.25 |
| Basicity milliequivalent/gram the solution of composition | ???0.055 | ??0.147 | ??-0.020 | ??0.202 | ??0.035 | ??0.127 | ??0.182 |
| Dipping experiment classification * | ????3 | ????5 | ????5 | ????3 | ????5 | ????5 | ????1 |
*1=is good, and 3=is general, and 5=is poor
These results show: contain TMAH, MEA and ascorbic acid as the best solution of cleaning agent performance (composition G) in the dipping experiment.The solution property that does not contain at least a these components is bad.These presentation of results are when TMAH, MEA and ascorbic acid coexist as in the cleaning solution, and when coexisting with preferred amounts especially, these components have the collaborative effect of cleaning.
Embodiment 4
Fig. 5 is illustrated in the AFM fractograph analysis of the through hole of 1 micron size on the original wafer surface.The degree of depth of through hole is about 400nm.The cross section test result of these through holes illustrates that clearly residue has the number of polymers residue after etching.
Prepare cleaning solution of the present invention, it consists of: the ascorbic acid of the TMAH of 10.0wt%, the MEA of 18.0wt%, 7.0wt% and the water of surplus.Down partially-etched through hole wafer is immersed in this solution 30 minutes at 70 ℃.Then with deionized water with about 1 minute of wafer rinsing, dry up with nitrogen then.
Fig. 6 illustrates the AFM fractograph analysis with the through hole of the same a kind of 1 micron size after the above-mentioned solution-treated.The cross-sectional view of these through holes shows their degree of depth very shallow (average 80nm).The difference of the degree of depth is that the thickness estimation of photoresist layer is about 300nm because removed the photoresist layer on the wafer surface before and after treatment.The via bottoms of rectangle (Fig. 6) illustrates that also lateral wall polymer removed by above-mentioned solution.These presentation of results embodiment preferred are to be applicable to that through hole cleans and the composition of cleaning photoresist.
Test the application of two kinds of solution in back CMP cleans.Solution I (gallic acid of the MEA of 0.45wt%, the TMAH of 0.25wt%, 0.175wt% and the water of surplus) and solution II (ascorbic acid of the MEA of 0.45wt%, the TMAH of 0.25wt%, 0.175wt% and the water of surplus) are used for cleaning experiment, with the Cobra-VcS station TEOS wafer that is immersed in the Olin Arch 10K slurries are carried out cleaning experiment.Fig. 7-8 illustrates the granule number in the wafer that cleans with the usefulness solution I of KLA-Tencor instrument test and solution II.Preferred composition-solution II of the present invention obviously has more superior cleaning performance.
Embodiment 6
Preparation is diluted to 1.25,1.33,2.5 and the concentrated solution of 5wt% and estimating respectively.(22 ℃ and 50 ℃) are immersed in these agitating solutions 30 minutes with the ECD of part complanation with wafer under two kinds of different constant temperatures.To carry out these handle before and carry out these wafers after handling and carry out the four point probe test, measure its sheet resistance.Estimate the copper rate of etch of these solution.Concentrate A is the ascorbic acid of MEA, 7.0wt% of TMAH, 18wt% of 10.0wt% and the water of surplus.Concentrate B is the gallic acid of MEA, 7.0wt% of TMAH, 18wt% of 10.0wt% and the water of surplus.Table IV illustrates the experimental result report with dust/minute expression.
| Table IV | ||||
| Concentrate composition A | Concentrate composition B | |||
| Concentration, wt% | Rate of etch in the time of 22 ℃ | Rate of etch in the time of 50 ℃ | Rate of etch in the time of 22 ℃ | Rate of etch in the time of 50 ℃ |
| ????1.25 | ?????4.52 | ?????23.35 | ?????22.05 | ?????88.39 |
| ????1.665 | ?????9.24 | ?????23.58 | ?????19.66 | ?????118.91 |
| ????2.5 | ?????0.55 | ?????24.68 | ?????28.86 | ?????161.39 |
| ?????5 | ?????0.00 | ?????13.91 | ?????27.82 | ?????234.20 |
Data from Table IV can be clear that: what the corrosion-inhibiting of concentrate composition A can be than concentrate composition B is good.
With two kinds of concentrated solutions of the method for embodiment 6 preparation and be diluted to 12.5 and 50wt% respectively.(22 ℃) are immersed in these agitating solutions 10 minutes with the ECD of part complanation with wafer under constant temperature.To carry out these handle before and carry out these wafers after handling and carry out the four point probe test, measure its sheet resistance.Table V illustrate with milliohm/centimetre
2The report that the sheet resistance of expression changes.
| Table V | ||
| Sheet resistance changes (Sheet Resistance Change) | ||
| Concentration wt% | Concentrate composition A | Concentrate composition B |
| ?????12.5 | ????-0.0015 | ????????0.1742 |
| ??????50 | ????-0.0994 | ????????0.3307 |
Can clearly be seen that: what the corrosion-inhibiting of concentrate composition A can be than concentrate composition B is good.Concentrate composition A also obviously has beat all effect, because sheet resistance decreases.
Invention has been described above, but the invention is not restricted to the described specific embodiments of the application, need be set in additional claims with the scope of protection of the patent right.
Claims (8)
1, a kind of cleaning solution that is used for the cleaning microelectronic substrate, this cleaning solution comprises:
The quaternary ammonium hydroxide that is selected from tetraalkylammonium hydroxide of 0.05-12.4wt%, alkyl wherein contains C
1-C
10A kind of or C in the atom
1-C
10Combination in the atom;
0.2-27.8wt% is selected from monoethanolamine, amino ethyl ethanolamine, N-methylaminoethanol, amino ethoxy ethanol, diethanol amine, triethanolamine, C
2-C
5The polarity organic amine of alkanolamine and composition thereof;
The corrosion inhibitor that is selected from ascorbic acid (vitamin C), L (+)-ascorbic acid, arabo-ascorbic acid, ascorbic acid derivates, BTA, citric acid, ethylenediamine tetra-acetic acid (EDTA) and composition thereof of effective dose; Water with surplus;
Wherein the basicity of solution is greater than 0.073 milliequivalent alkali/gram solution.
2, a kind of cleaning solution that is used to clean the cupric microelectronic substrate, this cleaning solution comprises:
The tetramethylammonium hydroxide of 0.5-12.4wt%;
The monoethanolamine of 0.2-27.8wt%;
The ascorbic acid of 0.2-10.9wt% and balance of deionized water;
Wherein the basicity of solution is greater than 0.073 milliequivalent alkali/gram solution.
3, according to the cleaning solution of claim 2, wherein the basicity of this solution is greater than about 0.1 milliequivalent alkali/gram solution.
4, according to the cleaning solution of claim 1, wherein said corrosion inhibitor is selected from ascorbic acid, L-ascorbic acid, arabo-ascorbic acid and ascorbic acid derivates.
5, a kind of cleaning solution that is used for the CMP cleaning, it is made up of the tetramethylammonium hydroxide of 0.05wt%-1.25wt%, the monoethanolamine of 0.2wt%-2.25wt%, the ascorbic acid of effective dose and the water of surplus basically.
6, a kind of through hole cleaning solution, it is made up of the tetramethylammonium hydroxide of 7.5wt%-12.4wt%, the monoethanolamine of 12.5wt%-27.8wt%, the ascorbic acid of 0.2wt%-10.9wt% and the water of surplus basically.
7, a kind of cleaning solution that is used for microelectronic substrate, this cleaning solution is made up of the concentrate of 1.5-12.5wt% and the deionized water of 87.5-98.5wt% basically, this concentrate is made up of following substances: the quaternary ammonium hydroxide that is selected from tetraalkylammonium hydroxide of 3.0-12.4wt%, alkyl wherein contains C
1-C
10A kind of or C in the atom
1-C
10Combination in the atom; 5.0-27.8wt% is selected from monoethanolamine, amino ethyl ethanolamine, N-methylaminoethanol, amino ethoxy ethanol, diethanol amine, triethanolamine, C
2-C
5The polarity organic amine of alkanolamine and composition thereof; Corrosion inhibitor that is selected from ascorbic acid (vitamin C), L (+)-ascorbic acid, arabo-ascorbic acid, ascorbic acid derivates, BTA, citric acid, ethylenediamine tetra-acetic acid (EDTA) and composition thereof and the surplus of 2.0-10.9wt% are water; The basicity of this solution is greater than 0.073 milliequivalent alkali/gram solution.
8, a kind of cleaning solution that is used to clean the cupric microelectronic substrate, this cleaning solution is made up of the concentrate of 1.5-12.5wt% and the deionized water of 87.5-98.5wt% basically, this concentrate is made up of following substances: the tetramethylammonium hydroxide of 5.0-12.4wt%, the monoethanolamine of 2.0-27.8wt%, the ascorbic acid of 2.0-10.9wt% and the water of surplus, the basicity of this solution is greater than 0.073 milliequivalent alkali/gram solution.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US09/587,883 | 2000-06-06 | ||
| US09/587,883 US6492308B1 (en) | 1999-11-16 | 2000-06-06 | Post chemical-mechanical planarization (CMP) cleaning composition |
| PCT/US2001/018402 WO2001095381A2 (en) | 2000-06-06 | 2001-06-06 | Post chemical-mechanical planarization (cmp) cleaning composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1433567A true CN1433567A (en) | 2003-07-30 |
| CN1205655C CN1205655C (en) | 2005-06-08 |
Family
ID=24351570
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB018107230A Expired - Lifetime CN1205655C (en) | 2000-06-06 | 2001-06-06 | Post chemical-mechanical planarization (CMP) cleaning composition |
Country Status (9)
| Country | Link |
|---|---|
| US (1) | US6492308B1 (en) |
| EP (1) | EP1287550B1 (en) |
| JP (1) | JP4942275B2 (en) |
| KR (2) | KR100831182B1 (en) |
| CN (1) | CN1205655C (en) |
| AT (1) | ATE462198T1 (en) |
| DE (1) | DE60141629D1 (en) |
| TW (1) | TW574369B (en) |
| WO (1) | WO2001095381A2 (en) |
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-
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- 2001-06-06 JP JP2002502824A patent/JP4942275B2/en not_active Expired - Fee Related
- 2001-06-06 AT AT01942043T patent/ATE462198T1/en not_active IP Right Cessation
- 2001-06-06 KR KR1020077026381A patent/KR100831182B1/en active IP Right Grant
- 2001-06-06 KR KR1020027016692A patent/KR100831180B1/en active IP Right Grant
- 2001-06-06 EP EP01942043A patent/EP1287550B1/en not_active Expired - Lifetime
- 2001-06-06 DE DE60141629T patent/DE60141629D1/en not_active Expired - Lifetime
- 2001-06-06 CN CNB018107230A patent/CN1205655C/en not_active Expired - Lifetime
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| CN106661518B (en) * | 2014-07-18 | 2020-01-14 | 嘉柏微电子材料股份公司 | Cleaning compositions for post-CMP use and methods relating thereto |
| CN106283097A (en) * | 2015-06-23 | 2017-01-04 | 易安爱富科技有限公司 | Cleaning liquid composition |
| CN106283097B (en) * | 2015-06-23 | 2018-12-04 | 易安爱富科技有限公司 | Cleaning liquid composition |
Also Published As
| Publication number | Publication date |
|---|---|
| DE60141629D1 (en) | 2010-05-06 |
| CN1205655C (en) | 2005-06-08 |
| KR100831182B1 (en) | 2008-05-22 |
| KR20030025238A (en) | 2003-03-28 |
| KR20070114326A (en) | 2007-11-30 |
| EP1287550B1 (en) | 2010-03-24 |
| ATE462198T1 (en) | 2010-04-15 |
| US6492308B1 (en) | 2002-12-10 |
| WO2001095381A2 (en) | 2001-12-13 |
| KR100831180B1 (en) | 2008-05-21 |
| JP2003536258A (en) | 2003-12-02 |
| EP1287550A2 (en) | 2003-03-05 |
| WO2001095381A3 (en) | 2002-05-23 |
| JP4942275B2 (en) | 2012-05-30 |
| TW574369B (en) | 2004-02-01 |
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